Methods for processing textile materials



pearance, hand and/or I I g 3,086,259 METHGDS FGR PRGCESSING TEXTILE AERIA Kermit S. La Fleur, Union, S.C., assignor to Deering MillikenResearch Corporation, Pendleton, 8.6., a corporation of Delaware NoDrawing. Fiied Dec. 9, 1957, Ser. No. 701,365

15 Claims. (Ci. 117-141) This invention relates to improvements intextile processing procedures and more particularly the inventionrelates to improved methods of lubricating, fulling and scouring textilefibers, yarns and fabrics of wool or mixtu'res of wool and othermaterials. 7

It is conventional practice to apply a lubricating material to woolfibers to assist in picking, carding, spinning, weaving and the like andmaterials which have been employed for this purpose include emulsifiablevegetable oils, mineral oils and mixtures of such oils. After thelubricating material has served its purpose, it is thereafter necessaryto remove the same with soap and/or a detergent since if even a smallquantity of the lubricating material is allowed to remain in thefinished fabric, it generally results in the fabric having anundesirable apodor and also interferes with the dyeing of the fabric.Generally, from about 4 to 6%, by weight of the wool, of lubricant isapplied and this is thereafter wasted since as yet no satisfactorymethod of recovering the lubricating agent in re-usable form has beendevised. In addition, conventional practice requires the use of 4% tosoap or detergent and 3% to 5% alkali, based on the weight of wool, toremove the lubri eating agent after it has served its purpose.

According to this invention, the waste inherent in prior art proceduresis eliminated, and improved results are otherwise obtained by applyingto the wool a small percent of a surface active agent, of a class to besubsequently defined, which is capable of acting as an excellentlubricating agent during carding, spinning, and weaving, a fulling agentduring fulling, and which is not only readily removed in scouring, butwhich actually assists in removing other soils that might be present onthe wool fiber. In other words, according to this invention, a singlematerial acts as lubricating, fulling and scouring agent.

The new procedure of this invention has several other importantadvantages, and a first such advantage is that even if scouring is noteifective in completely removing the processing agent from the wool, thesurface active lubricants employed in the process of this invention donot materially interfere with the dyeing procedure. Prior to thisinvention, inadequate scouring has been a frequent cause of difiicultysince it is generally impossible to eifect even and complete removal ofthe lubricating agent from the fabric and even small amounts ofconventional lubricants remaining in the fabric can result in unevendyeing o-r shading. When, however, woolen materials are processedaccording to this invention, any lubricant remaining in the fabric atthe time of the dyeing operation seems to be uniformly distributed andcauses no diiiculty.

Another important advantage of this invention is that smaller quantitiesof lubricant can be used because of the high degree of effectiveness ofthe class of materials employed. In other words, the process of thisinvention not only eliminates the use of detergents and/or alkalies toremove the spinning oil from thetextile fibers, but also eliminates thenecessity of empolying such quantities of a lubricant in the firstinstance.

Still another advantage of the invention is that it simplifies problemsof inventory and requires the stock- 'of only one material. The priorart process has'heretof're required that a supply of at least two or.three materials be maintained and the new process of "this taes tnt3,689,259 Patented Mar. 5, 1963 ice 2 invention eliminates theadministrative work normally necessary for making certain that adequatesupplies of the several materials are on hand at all times.

A further advantage of the new process of this invention is that itpermits the use of conditions which result in less damage to the woolfibers. It is Well known by those skilled in the art that subjectingwool fabrics to highly alkaline conditions results in damage to the woolfibers and yet prior to this invention, the use of a very alkaline andhigh temperature bath for scouring has generally been necessary tocompletely remove the lubricant conventionally applied to wool fibers.Numerous efforts have been made to employ acid or relatively neutralconditions in securing but such procedures have not been widely employedbecause it is quite diiiicult to obtain a completely satisfactory handunder such conditions. According to the process of this invention thefulling and scouring operations can be conducted at any desired pH.

A still further advantage of the new process of this invention is thatit permits goods to be carbonized in the grease with less discolorationthan when conventional lubricants are employed. In many instances,carbonizing in the grease permits an overall simplification of theproduction procedure but prior eiforts to carbonize before scouring haveresulted in yellowing of the textile material to an extent which makesit unsuitable for light shades. By the process of this invention thetextile material can be carbonized in the grease and still retain asatisfactory degree of whiteness.

The class of materials which are employed as processing agents accordingto this invention, are high molecular weight, water-dispersable, aminebases, and acid addition salts thereof, said bases being capable ofbeing represented by the formula:

alt t z i n -nikmt( z imy nz wherein N is the symbol for nitrogen; C isthe symbol for carbon; H is the symbol for hydrogen; 0 is the symbol foroxygen; R represents a hydrophobic group; R and R in each instance,represent hydrogen or blocking groups; R represents a divalenthydrocarbon connecting radical having from 1 to 6 carbon atoms; x and yrepresent integers of from 0 to 8 in each instance and the total of allxs and all ys is from 3 to 8; and n represents an integer from 0 to linclusive. Mixtures of amine bases of the above formula and/ or of acidaddition salts thereof can be suitably employed and, in fact, thepreferred processing agents according to this invention are generallymixtures, since it is exceedingly difficult and unnecessarily expensiveto prepare compounds of the above formula in pure form.

The nature and length of the hydrophobic group in compounds of the aboveformula are quite important since both the length of the group and itschemical nature affect the properties and partially determine thesuitability of the compounds for use according to this invention. Afirst important consideration is that the length and nature of the groupmust be balanced against the number of oxyethylene groups in thecompound so that the compound is readily water dispersable, but nottruly water soluble. In other words, the hydrophile-lipophile balance ofthe compound must be such that it will readily "form an aqueousdispersion which is stable for at least upon the hydrophobic group ispermissible although it reduces the hydrophobic nature of the group andrequires that the compound have a smaller number of oXyethylen-e groupsthan would otherwise be most advantageous. The hydrophobic group is alsopreferably saturated since it has been found that compounds containing ahigh degree of unsaturation are not so effective as lubricants, althoughthe hydrophobic group may be ethylenically unsaturated at l or 2 pointswithout destroying the lubricity of the compound and in certaininstances compounds having a small degree of unsaturation might bepreferred because of their liquid form at room temperature. Straightchain hydrophobic groups are generally preferred to branched chainaliphatic radicals. All of these factors not only affect the lubricityof compounds of the above formula but, at least in some instances, alsohave an effect upon the total number of carbon atoms which may besuitably present in the hydrophobic group. As a general rule, however,the number of carbon atoms in the hydrophobic group can suitably rangefrom to 20 with the preferred number being from 14 to 18.

The radical represented by R in the above formula is a divalentaliphatic hydrocarbon connecting radical having from 1 to 6 carbonatoms. t will be apparent from the formula that R can either link thehydrophobic group R to the terminal amine group through an intermediateamine group or can directly link the group R to the terminal amine groupthrough a carbon to carbon linkage and that in the latter instance, Rand R may suitably be considered as a single hydrophobic radical. in anyevent, R also has a hydrophobic influence and its length partiallydetermines the optimum number of carbon atoms in the primary hydrophobicgroup represented by R In instances where R links the primaryhydrophobic group R to the terminal amine group through an intermediateamine group, R preferably represents an ethylene group and partiallyoffsets the hydrophilic effect of the intermediate amine group, and ininstances where R directly links 1x1 to the terminal amine group, Rpreferably represents a methylene group so that the total number ofcarbon atoms in R and R is from 15 to 19.

Compounds of the above formula containing only one amine group aregenerally preferred and, as a rule, give better results than compoundscontaining two amine groups. If the compound contains only one aminegroup, however, it is generally necessary that it contain a largernumber of oxyethylene groups than when the surface active agent containstwo amine groups, since the compounds employed in the process of thisinvention should be water-dispersable and an amine group acts as a watersolubilizing group. With compounds containing a single amine group, thetotal number of oxyethylene groups should normally be from 3 to 8, withthe preferred number depending upon the nature of the aliphatic chain.In the instance of a compound containing a single amine group and inwhich the hydrophobic radical (R -H1 is an octadecyl radical, thepreferred number of oxyethylene groups is 5. in the case of compoundscontaining two amine groups, the total number of oxyethylene groups isgenerally from 2 to 5, with the preferred number being 3 in the case ofa compound in which the hydrophobic radical R is an octadecyl radicaland the connecting radical R is an ethylene radical. The oxyethylenechains in compounds suitable for use in this invention can terminate infree hydroxy groups or in hydroxy groups blocked by transformation intolower alkoxy groups, such as methoxy and ethoxy, or lower fatty acidacyloXy groups as illustrated by acetoxy and formoyl groups.

Specific examples of compounds which can suitably be employed in thisinvention include the following:

Compounds of this type can be prepared by procedures well known in theart and several mixtures, containing compounds of the above type andsuitable for use in this invention, are commercially available.

The processing agent of this invention can be applied at any stage ofoperations where a lubricant, fulling agent or scouring agent isconventionally applied since it serves to replace all such agentsemployed in prior art procedures. For example, a small amount of theprocessing agent can advantageously be applied at the picker tolubricate the fibers during picking, carding, spinning, and weaving. Anadditional quantity of the processing agent can advantageously beapplied immediately before or during fulling since if sutficientlubrication is applied prior to falling to give the best results in thisoperation, it is generally in excess of the amount necessary for bestlubrication of the fibers during picking, carding, spinning, andweaving.

The amount of the processing agent most advantageous ly applied at thepicker depends upon a number of factors, foremost among which is theamount of natural oils in the fibers, but generally a suitable amount ofthe processing agent will vary from 0.1% to 5% with the preferred rangebeing from 1% to 2%. It will be noticed that this is considerably belowthe amount of wool oil conventionally applied at this point since atleast about 5% of a conventional Wool oil is normally required for bestresults. The processing agent is preferably applied at this point in theform or" an aqueous dispersion since a dispersion enables one to make arelatively even application of the processing agent, and the Water inthe dispersion acts to hold down fly. A dispersion having aconcentration varying within wide limits can suitably be employed andthe only important considerations are that the dispersion be not soconcentrated that an even application of the processing agent isdil'licult, nor so dilute that it is necessary to make the stock too wetin order to apply a satisfactory amount of the processing agent. As ageneral rule, a suitable concentration for the aqueous dispersion to beapplied at the picker is from 3% to 30% with the preferred concentrationbeing from 5% to 15% by weight. The aqueous dispersion may be applied byany suitable means and, for example, may be sprayed onto the stock froma nozzle or applied by means of an absorbent roll or the like.

It is generally advantageous to apply an additional quantity of theprocessing agent immediately preceding or during fulling to therebyprovide better fulling and more effective scouring, and except foreconomic considerations, there is practically no upper limit as to theamount of the processing agent that can be applied at this point. Onecan, for example, apply an additional 20% of the processing agent atthis point with satisfactory results but such a large amount of theprocessing agent is completely unnecessary and it is seldom, if ever,advantageous to apply more than about 5% of the processing agent duringor immediately before fulling. The preferred amount of the agent to beemployed at this time, assuming that the fabric already contains from 1%to 2% of theprocessing agent previously applied for purposes of fiberlubrication, is from about 0.5% to 3% based upon the weight of thegoods. Of course, if the fabric contains less than about 1% of aprocessing agent according to this invention due to the fact that aconventional lubricant was employed, alone or in combination with anagent according to this invention, for fiber lubrication in thepreceding processing operation, or due to the fact that part of theagent previously applied has been removed, or for any other reason,larger amounts of the processing agent are generally advantageous, andan amount of the agent should be applied to bring the total amount ofthe agent present in the fabric up to at least about 1.5% to 5% byweight. The processing agent is also, in this instance, preferablyapplied in the form of an aqueous dispersion and again the concentrationof the dispersion is relatively unimportant. Under proper conditions, adispersion of the processing agent having a concentration of from 0.1%to 60% by weight can be employed, but there is a wcllrecognized optimummoisture content for fulling, and it is generally advantageous to employa dispersion of a proper concentration to furnish the desired quantityof water for the fulling operation. Since an optimum moisture contentfor fulling is generally from 50% to 100% by weight of the goods, andsince it is generally advantageous to add from about 0.5% to 3% of theprocessing agent, it will be seen that the preferred concentration forthe aqueous dispersion to be employed immediately before falling is fromabout 0.5% to 6%. The dis persion of the processing agent can be appliedbefore or during falling by any suitable means but a preferred procedurecomprises applying the agent by means of a conventional soaper beforethe fabric is placed in the fulling mill.

A dispersion suitable for use in this invention can be readily preparedsince the processing materials are readily water dispersable and in mostinstances no special apparatus is required. Some agitation is, ofcourse, advantageous to insure uniformity of the dispersion, and in someinstances better results are achieved if the water employed in formingthe dispersion is heated, for example, to from 60 to 95 0., but in mostinstances all that is necessary is for the processing material to beadded to a calculated amount of water to give a dispersion of thedesired concentration and the resulting mixture slightly agitated.

Because the processing agents of this invention are readily waterdispersable and do not interfere with dyeing when present in the dyebath in limited quantities, it is frequently possible to eliminate thescouring operation which conventionally precedes dyeing, and this isparticularly true when the goods are of the type which are not subjectedto a fulling operation. Fabrics formed from halogenated wool fibers andfabrics formed from a blend of wool with at least about 50% of anon-falling fiber material such as nylon fibers, Dacron polyesterfibers, or Orlon and Acrilan acrylic fibers, do not full and need not besubjected to a fulling operation. When employing a processing agentaccording to this invention, the conventional scouring operation canalso be eliminated and the fabric can be taken directly from the loom tothe dye bath.

Conventional temperatures can be employed in the process of thisinvention although it is an advantage of the invention that the scouringoperation can be conducted at room temperature. If the wool iscontaminated with relatively large amounts of soil, it has been foundthat improved scouring is obtained if the bath is slightly Warm and forthis reason, a temperature of about 100 F. is generally preferred forscouring.

It is also an advantage of the invention that no pH adjustments arerequired in either the fulling or scouring operations. The aminesemployed in the new process of this invention are normally basic andgive an unadjusted pH of about 9 or 10 in aqueous solution and generallyit is advantageous to conduct both the fulling and scouring operationsunder such basic conditions Without pH adiustment. If desired, however,both the fulling and scouring operations can be conducted under neutralor acidic conditions. For example, the dispersion applied immediatelybefore or during fulling can he neutralized with an organic acid, suchas acetic or formic, or with a non-oxidizing mineral acid, such assulfuric acid or hydrochloric acid, before it is applied to thematerial, or an acid addition salt of the amine base can be em.- ployedin forming the dispersion. Likewise, an acid may be added to the bathemployed in the securing operation in amounts sufficient to result inthe bath being made neutral or acidic since it is a characteristic ofthe materials employed in the process of this invention that theypossess a greater degree of detergency when in the form of acid additionsalts than when in the form of free bases.

The invention will now be illustrated by the following specificexamples, in which all parts are by weight onless otherwise indicated:

Example I To a wool blend consisting of 40% 12-month Texas wool, 20% NewMexican wool, 20% 8-month Texas wool, and 20% fine Lister Noils (noilsfrom a Lister comb), there is applied a 7 /2% aqueous dispersion of amixture of amines of the formula:

wherein m and n represent integers with the average total of m and nbeing about 5, and R represents octadecyl, in most instances, withsmaller amounts of compounds wherein R represents cetyl, and oleyl alsobeing present. An amount of the dispersion is applied such that about1.75% of the amine mixture is deposited on the wool and the wool is thenpicked, carded, spun into a variety of yarn weights and woven into plainweave woolen fabrics. In comparative tests on 20 pieces of fabric thusprepared, four pieces were fulled and scoured with the addition of wateronly and were thereafter carbonized, rinsed, and dyed; four pieces weresc aped with an additional 1.25% of the above amine mixture (bringingthe total to 3%), fulled, scoured, carbonized, rinsed, and dyed; eightpieces were soaped with an additional 1.25% of the amine mixture,fulled, scoured, with the addition of 1% acetic acid, carbonized,rinsed, and dyed; and four pieces were crabbed, carbonized, soaped with1.25% of the amine mixture (total used 3%total presout about 2%),fulled, scoured, and dyed. All 20 pieces were satisfactory, but thefulling operation gave better results when at least about 2% of theamine mixture was present on the fabric.

In this instance comparative tests were also made using, in place of1.75% of the amine mixture, 5% of a standard and well-accepted mineraloil lubricant (Twitchel 7421 wool oil) for the picking, carding,spinning, and weaving operations. A smaller reduction in average fiberlength during car-ding was experienced when employing the mixture ofamines than when employing the standard mineral oil lubricants (the meanreduction in fiber length when employing the amine mixture was 0.1 inch,while the mean reduction in fiber length when employing the mineral oillubricant was 0.28 inch), and during spinning there were only 107 breaksper thousand spindle hours for 9.15 thousand spindle hours in the caseof fibers lubricated with the amine mixture, whereas there were breaksper thousand spindle hours for 11.7 thousand spindle hours in the caseof fibers lubricated with the standard mineral oil lubricant.

Example I! To a W001 blend containing 45% wool and 55% Nylon 66 fibersthere is applied approximately 25% of a 7% ass-ass i? in which R' ineachinstance represents either hydrogen, hy'droxyethyl, or apolyoxyethylene subsituent 1L6.

C H O-C H OH or C H O C H OH with'the av'erage'total number ofoxyethylene groups being 3, and R represents octadecyl in most instanceswith smaller amounts of compounds also being present in which Rrepresents a cetyl, or an oleyl group. The Wool mixture is then picked,carded, spun, woven, and dyed with the fabric being taken directlyfromthe loom to the dye beck. The dyedfabric is substantially free ofobjectionable shading and is' otherwise satisfactory.

The procedure when employing other processing agents according to thisinvention is the same as in the above examples. p V

Having thus'described'rny invention, what I desire to claim and secure"by Letters Patent is;

V 1. In the processing ot a textile material comprising wool fiberswherein said material is subjectedto the processing operations ofpicking, carding; spinningweaving, fulling and scouring; the improvementwhich comprises applying to the textile material prior to picking, asthe sole essential processingyagent acting as a lubricating agent,fulling agent and scouring agent, a composition select-ed from the groupconsisting of amines capable of being represented by the formula:

wherein R represents a hydrophobic radical having from 10 to 20 carbonatoms and is selected from the group consisting of hydrocarbon nadicalsand hydroxy substituted hydrocarbon radicals; R and R in each instance,represent a'member selected-from the group consisting of hydrogen, loweralkyl'r'adicals, and lower fatty acid acyl radicals; R represents adivalent hydrocarbon connecting radical having from 1 to 6 carbon atoms;x and y represent intege'rsof from to 8 in each instance and thetotal-of all xs and 'all ys is from 3 to- 8; and n represents an integerfrom 0 to 1 inclusive, the hydr'ophilelipophile balance of said'aminebeing such that it is readily water dispersibie but will not readilyform a molecular solution in water; acid addition salts of such amines,and mixtures thereof.

2. The improvement of'claim '1 wherein the processing agent is appliedin an amount from about 0.01 to about 5%, based on the weight of thetextile material.

3. The improvement of claim 2 wherein the amount of said' processingagent applied is from 1% to 2%.

4. The improvement of claim 2 wherein an additional quantity of saidprocessing agent is applied immediately prior to fullingto assist in thefulling and scouring operanions.

5,. The improvement" of claim 4 wherein the amount of said processingagent applied immediately prior to fulling is from 0.5% to 6%, based onthe dry weight of said textile material.

6. The improvement of claim 4 wherein said processing agent comprises analiphatic mono-amine in which the amino group has at least onepolyoxyethylenc hydrophilic substituent, the total mean number ofoxyethylene' groups in said amine being from 3 to 8 inclusive.

7. The improvement of claim 6 wherein said aliphatic monoernine'has theformula }CHT"CH2O)nH R-N (CHPOHPOMDE wherein R is selected from thegroup consisting of octadecyl, cetyl and oleyl and wherein m and 11represent integers with the average of m and n being' about 5.

8. The improvement of claim 6 wherein said amine has an octadecylsubstituent;

9. The improvement of claim 8 wherein the total mean number ofoxyethylene groups in said amine is 5'.

10. The improvement of claim 4 wherein said processing agent comprisesan e-thylenediamine in which one of the amino groups is substituted'witha hydrophobic aliphatic radical and the compound contains at least onehydrophilic oxyethyl'ene substituent, the total means number ofoxyethylene' groups in'sa'id amine being from 2'to' 5 inclusive.

11. The improvement of claim 10 wherein said proc'- essingagent'compr-ises an ethylen d-i-amine having the formula wherein R isselected from the group consisting of octadecyl, cetyl and oley-l andwherein R is selected from the group consisting of. hydrogen,hydroxyethylene, 'C21 the average number of the oxyethylene groupspresent being3.

12. The improvement of claim 10 wherein said hydrophobic radical is anoctadecyl radical-and the total means number of oxye'thylene groups insaid amine is 3.

13. A method for processing a textile material composed of a memberselected from the group consisting of blends of wool with syntheticfibers, halogenated wool fibers, and mixtures thereof, which comprisesapplying to said textile material from about 0.1% to 5% of a processingagent consisting essentially of a member se lected from the groupconsisting ofarnines capable of being representedby the formula:

1 a 4 x 2] n 3 2 4 y 4] 2 wherein R represents a hydrophobic radicalhaving from 10 to 20 carbon atoms andis selected from the groupconsisting of hydrocarbon radicals and hydroxy substituted hydrocarbonradicals; R and R in each instance, represents a member selected fromthe group consisting of hydrogen, lower alkyl radicals, and lower fattyacid *acyl radicals; R represents a divalent hydrocarbon connect ingradical having from 1 to 6- carbon atoms; x and 3* represent integers offrom 0 to 8 in each instance and the total of all xs and all ys is from3 to 8; and n represents an integer'frorn 0 to 1 inclusive, thehydrophile-lipophile balance of said amine being such that it is readilywater dispersible but will not readily form a molecular solution inwater; acid addition salts of such amines, and mixtures thereof, andthereafter subjecting said textile material to the operations ofpicking, carding, spinning, weaving, and dyeing without an intermediatescouring operation.

14. A process according to claim 13 wherein said processing agentcomprises an alkyl amine having at least one hydrophilic oxyethylenesubstituent, the total mean number of oxyethylene groups being from 3 to8 inclusive.

-15. The improvement of claim 14 wherein the alkyl group in said amineis an octadecyl radical,

References tilted in the file of this patent UNITED STATES PATENTS 7 Re.17,264 Schaefer ..'Apr. 9, 1929 2,387,510 Heintz et al Oct. 23, 19452,809,159 Welles et al Oct. 8, 1957 2,857,330 Hall Oct. 21, 19582,877,178 Bergman 'et al Mar. 10, 1959 2,925,639 La Fleur Feb. 23, 196-0OTHER REFERENCES ,lrocessing Du Pont' Nylon Staple on' the WoolenSystern, Bulletin N-31, November 1955.

1. IN THE PROCESSING OF A TEXTILE MATERIAL COMPRISING WOOL FIBERSWHEREIN SAID MATERIAL IS SUBJECTED TO THE PROCESSING OPERATIONS OFPACKING, CARDING SPINNING WEAVING FULLING AND ACOURING, THE IMPROVEMENTWHICH COMPRISES APPLYING TO THE TEXTILE MATERIAL PRIOR TO PACKING, ASTHE SOLE, ESSENTIAL PROCESSING AGENT ACTING AS A LUBRICATING AGENTFULLING AGENT AND SCOURING AGENT, A COMPOSITION SELECTED FROM THECONSISTING OF AMINES CAPABLE OF BEING REPRESENTED BY THE FORMULA: